CN101657522A - The pressure sensitive adhesive of antistatic optically clear - Google Patents

The pressure sensitive adhesive of antistatic optically clear Download PDF

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Publication number
CN101657522A
CN101657522A CN200880011906A CN200880011906A CN101657522A CN 101657522 A CN101657522 A CN 101657522A CN 200880011906 A CN200880011906 A CN 200880011906A CN 200880011906 A CN200880011906 A CN 200880011906A CN 101657522 A CN101657522 A CN 101657522A
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China
Prior art keywords
tackiness agent
salt
methyl
agent according
adhesive
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Granted
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CN200880011906A
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Chinese (zh)
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CN101657522B (en
Inventor
艾伯特·I·埃费拉茨
夏剑辉
尹万植
朱东伟
威廉·M·拉曼纳
托马斯·P·克伦
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3M Innovative Properties Co
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3M Innovative Properties Co
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04—Homopolymers or copolymers of esters
    • C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/062—Copolymers with monomers not covered by C09J133/06
    • C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04—Homopolymers or copolymers of esters
    • C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2666/00—Composition of polymers characterized by a further compound in the blend, being organic macromolecular compounds, natural resins, waxes or and bituminous materials, non-macromolecular organic substances, inorganic substances or characterized by their function in the composition
    • C08L2666/02—Organic macromolecular compounds, natural resins, waxes or and bituminous materials
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2323/00—Functional layers of liquid crystal optical display excluding electroactive liquid crystal layer characterised by chemical composition
    • C09K2323/03—Viewing layer characterised by chemical composition
    • C09K2323/031—Polarizer or dye
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
    • Y10T428/2848—Three or more layers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
    • Y10T428/2852—Adhesive compositions
    • Y10T428/2878—Adhesive compositions including addition polymer from unsaturated monomer
    • Y10T428/2891—Adhesive compositions including addition polymer from unsaturated monomer including addition polymer from alpha-beta unsaturated carboxylic acid [e.g., acrylic acid, methacrylic acid, etc.] Or derivative thereof

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Polarising Elements (AREA)

Abstract

The invention provides optically transparent indicating meter level tackiness agent, described tackiness agent comprises: (a) crosslinked acrylic psa, (b) organic soluble and can dissociated salt, with optional (c) non-hydrophilic plasticizer, wherein said tackiness agent be electrostatic dissipation and be the low haze transmission to visible light.The method for preparing and use described tackiness agent also is provided in addition.

Description

The pressure sensitive adhesive of antistatic optically clear
CROSS-REFERENCE TO RELATED PATENT
The application requires the U.S. Provisional Patent Application No.60/911 of submission on April 13rd, 2007,800 right of priority, and the disclosure of this patent is incorporated this paper into way of reference in full.
Technical field
The present invention relates to pressure sensitive adhesive (OCA) composition of antistatic optically clear.Anti-electrostatic OCA disclosed in this invention can be used for (for example) liquid crystal display assembly, with polaroid bonding to liquid crystal cell.
Background technology
In liquid-crystal display (LCD) was used, optically transparent pressure sensitive adhesive (OCA) can be used for polaroid is adhered to liquid crystal cell.Polaroid can be for any type, for example H polaroid and K polaroid.Polaroid can directly contact or indirect contact with OCA.The skin of liquid crystal cell is generally glass.The basic demand that is used for the OCA of this LCD application comprises high optical clarity, low haze and low birefringence.
OCA is provided on the antiseized liner of tackiness agent usually.When adhesive surface removes antiseized liner, may on tackiness agent, stay the remaining static charge of several hectovolts.So big electric charge may the orientation to liquid crystal have a negative impact when OCA is coated to liquid crystal cell, and perhaps this electric charge may damage electronic circuit, therefore, this residual charge must be reduced to harmless level before OCA is coated to liquid crystal cell.
Existing people advises using conductive adhesive and anti-electrostatic liner to reduce or eliminate the disadvantageous effect of residual charge.Known electroconductibility pressure sensitive adhesive also can anti-electrostatic, the partial electric charge because it can dissipate easily.Yet this conductive adhesive uses the particle of conduction, for example glass microballon of carbon fiber, nickel particles or metallizing.The particle of this conduction is painted or even as big as scattered light, and these conductive adhesives are not optically transparent.Can realize antistatic property by being positioned at conductive coating on the pressure sensitive adhesion tape backing surface or that be positioned on tackiness agent self surface.For example, can prepare pressure-sensitive band of anti-electrostatic or sheet by between tackiness agent and band backing, using the vanadium pentoxide conductive coating.
Yet,, arrange that between tackiness agent and band backing conductive coating can not make the electric charge on the adhesive surface discharge rapidly, and only make tackiness agent have the electrostatically dissipative of some degree because tackiness agent is not good charged particle carrier usually.Can predict, binder layer thickness is big more, and charge dissipation is slow more.In addition, the antiseized liner realization of the anti-electrostatic electrostatically dissipative that has tackiness agent by use.Electric charge on this antiseized liner that can dissipate, but a large amount of electric charges on adhesive surface, still kept.
Summary of the invention
The invention solves this needs, a kind of pressure sensitive adhesive of antistatic optically clear is provided.This tackiness agent is in can be used for (for example) LCD application.In some applications, this OCA also should be insensitive and stable in high temperature and/or high humidity environment to moisture.
In some applications, the laminated thing of polaroid OCA should be reprocessed.For example, in the LCD component application, removing polarization layer may be ideal or necessity, for example when initial structure does not reach requirement fully.In this case, the adhesion level of anti-electrostatic OCA must allow polaroid to separate with LCD under the condition of not damaging LCD.Thereby the initial adherence force level of anti-electrostatic OCA should be enough to keep assembly together, and still, this adhesion level should not passed in time and is increased to high reprocessing extremely if desired, may damage the level of LCD when removing polarization layer.In addition, anti-electrostatic OCA should have enough bond strengths, makes not stay resistates when removing tackiness agent and polaroid on LCD.In addition, the OCA bond strength should not exceed the tearing strength of polaroid, makes polaroid and tackiness agent to be removed together and do not tear polaroid.
Thereby, the invention provides a kind of tackiness agent with antistatic optically clear of excellent surface conductivity (it can provide with good volume conductivity).Use the tackiness agent of these novel antistatic optically clears, can dissipate rapidly is positioned at static charge on the adhesive surface, and can eliminate basically in the assembling process because the LCD fault of electrostatic discharged initiation.
In brief, the invention provides a kind of optically transparent indicating meter level tackiness agent, described indicating meter level tackiness agent comprises crosslinked acrylic psa, organic soluble and can dissociated salt and optional non-hydrophilic plasticizer, wherein this tackiness agent be electrostatically dissipative and transmission of visible light is at least about 80%, at least about 85% or even at least about 90%, and mist degree is lower than about 15%, about 10%, about 8% even about 5%.
On the other hand, the invention provides a kind of method for preparing optically transparent indicating meter level tackiness agent, described method comprises provides at least a acrylic monomer and optional at least a comonomer; With this monomer and organic soluble and can dissociated salt and the linking agent blend to form the adhesive precursor composition; This adhesive precursor composition is provided on the first antiseized liner; And activate this linking agent to form crosslinked acrylic psa, wherein this tackiness agent is an electrostatically dissipative, and randomly, wherein the transmission of visible light of this tackiness agent be at least about 80%, at least about 85% or even at least about 90%, and level of haze be lower than about 15%, be lower than about 10%, be lower than about 8% even be lower than about 5% mist degree.
On the other hand; the invention provides a kind of multilayer polaroid; described multilayer polaroid comprises crosslinked acrylic psa; this crosslinked acrylic psa comprises can dissociated organic soluble salt; and choose wantonly and comprise non-hydrophilic plasticizer; wherein this tackiness agent is an electrostatically dissipative, and wherein this polaroid also comprises and is selected from anti-one or more layers of dazzling in photosphere, protective layer, reflecting layer, phase delay layer, wide-angle layer of compensation and the brightness enhancing layer.
On the other hand, the invention provides liquid-crystal display, described liquid-crystal display comprises crosslinked acrylic psa, this crosslinked acrylic psa comprises can dissociated organic soluble salt, and choose wantonly and comprise non-hydrophilic plasticizer, wherein this tackiness agent is an electrostatically dissipative with polaroid and liquid crystal cell, chooses wantonly and wherein all provides this tackiness agent in the liquid crystal cell both sides.
On the other hand, the invention provides a kind of method for preparing optically transparent indicating meter level tackiness agent, described method comprises: slurry is provided, and this slurry is by being mixed with acrylic polymers and at least a acrylic monomer and optional at least a comonomer; With this slurry and light trigger, organic soluble and can dissociated salt, linking agent and optional softening agent blend to be to form the adhesive precursor composition; This adhesive precursor composition is provided on the first antiseized liner; And the activation light initiator to be to form crosslinked acrylic psa, and wherein this tackiness agent is an electrostatically dissipative.
In presents, " (methyl) acrylic acid groups " comprises acrylic acid groups and methacrylic acid group, " (methyl) acrylic ester polymer comprises acrylic ester polymer and methacrylate polymers ", " replacement " means by the conventional substituting group that does not disturb required product and replaces, for example, substituting group can be alkyl, alkoxyl group, aryl, phenyl, halogen (fluorine, chlorine, bromine, iodine), cyano group, nitro or the like, and " electrostatically dissipative " means the surface resistivity of sample less than 10 13Ohm-sq.
In presents, " non-wetting ability " is meant the material that can absorb the moisture that is less than himself weight from its environment.
The advantage of one or more embodiment of the present invention has provided the tackiness agent with enough surface conductivities and enough conductive antistatic optically clears of volume, with the static charge that dissipates and produce when tackiness agent removes the antiseized liner that supports tackiness agent at a high speed.In addition, the tackiness agent of one or more embodiment of the present invention be for reprocessing, so that the polaroid that connects this tackiness agent can be removed neatly from LCD glass, for example can be used on the LCD assembling and handles the back when finding laminated defective.In addition, the OCA bond strength should not exceed the tearing strength of polaroid, makes polaroid and tackiness agent to be removed together and do not tear polaroid.The adhesion of the tackiness agent of one or more embodiment of the present invention is enough to suppress that the LCD polaroid takes place not expect peels off, minimizes the bubble between polaroid and the glass and make and only shrink on minimum degree ground at environment loop test rear polarizer.In addition, disadvantageous interaction does not take place in the tackiness agent of one or more embodiment of the present invention and LCD polaroid.
According to following embodiment and claim, further feature and advantage will be apparent all.Above summary of the invention is not that intention is described each illustrated embodiment of the present invention or every kind of embodiment.More particularly, following embodiment illustrates the presently preferred embodiment that some uses principle disclosed herein.
Embodiment
All numeral supposition herein all can be modified by term " about ".Numerical range with the end points statement comprises all numerals (for example, 1 to 5 comprises 1,1.5,2,2.75,3,3.80,4 and 5) that comprise in this scope.Except as otherwise noted, otherwise the percentages of quantity of material.
The invention provides a kind of optically transparent indicating meter level tackiness agent, this tackiness agent comprise crosslinked acrylic acid polymer, can dissociated organic soluble salt and optional non-hydrophilic plasticizer, wherein this optically transparent indicating meter level tackiness agent is pressure-sensitive and electrostatically dissipative.
Pressure sensitive adhesive
Any suitable contact adhesive composition all can be used for the present invention.In specific embodiment, tackiness agent is pressure-sensitive with optically transparent.Pressure sensitive adhesive (PSA) is known by the people to have following characteristic: (1) at room temperature strong even persistent viscosity, (2) adhere to substrate being no more than under the finger pressure, (3) be enough to remain on ability on the adherend, and/or (4) are enough to the bond strength that totally removes from adherend.In addition, this pressure sensitive adhesive can be the combination of single tackiness agent or two or more pressure sensitive adhesives.
Measure on 25 microns (μ m) thick sample with the method that describes below, if tackiness agent show at least about 90% or even higher optical transmittance and be lower than about 5% or even lower haze value, then be considered as optically transparent.The available pressure sensitive adhesive comprises (for example) polyvinyl ether, poly-(methyl) acrylate (comprising acrylate and methacrylic ester) among the present invention.
Available alkyl acrylate (being alkyl acrylate monomer) comprises the monofunctional acrylate or the methacrylic ester of the non-tert-alkyl alcochol of straight or branched, and its alkyl has 1 to 14 carbon atom, particularly 1 to 12 carbon atom.The available monomer comprises (methyl) butyl acrylate, (methyl) 2-EHA, (methyl) ethyl propenoate, (methyl) methyl acrylate, (methyl) vinylformic acid n-propyl, (methyl) isopropyl acrylate, (methyl) vinylformic acid pentyl ester, (methyl) vinylformic acid n-octyl, (methyl) Isooctyl acrylate monomer, (methyl) vinylformic acid ester in the different ninth of the ten Heavenly Stems and (methyl) vinylformic acid 2-methyl butyl ester.
In one embodiment, pressure sensitive adhesive is based at least a poly-(methyl) acrylate (for example being (methyl) acrylic psa).Gather (methyl) acrylic psa derived from (for example) at least a (methyl) alkyl acrylate monomer, for example Isooctyl acrylate monomer, vinylformic acid ester in the different ninth of the ten Heavenly Stems, vinylformic acid 2-methyl butyl ester, 2-EHA and n-butyl acrylate, isobutyl acrylate, Ethyl acrylate, vinylformic acid n-octyl, n octyl methacrylate, vinylformic acid ester in the positive ninth of the ten Heavenly Stems, vinylformic acid isopentyl ester, vinylformic acid ester in the positive last of the ten Heavenly stems, isodecyl acrylate, isodecyl methacrylate and dodecyl acrylate; With at least a optional comonomer composition, for example (methyl) vinylformic acid, N-vinyl pyrrolidone, N-caprolactam, N, N-dimethyl (methyl) acrylamide, N-sec.-propyl (methyl) acrylamide, (methyl) acrylamide, isobornyl acrylate, vinylformic acid 4-methyl-2-pentyl ester, (methyl) acrylic acid hydroxy alkyl ester, vinyl ester, polystyrene or polymethylmethacrylate macromole, toxilic acid alkyl ester and fumaric acid alkyl ester (respectively based on toxilic acid and fumaric acid) or their combination.
The OCA of various embodiment can be removable and/or can reprocess, or persistent relatively, makes that OCA's removes the adherent substrate of damage.This OCA for example comprises the acrylic monomer of carboxylic acid, acid amides, carbamate, urea or hydroxy functional group derived from least a (methyl) alkyl acrylate and optional polar monomer.In weak polar monomer such as N-vinyl lactam also can be included in.Also can use the combination of these polar monomers.In general, the polar monomer content among the OCA in total polymer content less than about 5%.Preferably, polar monomer content is about 3% or still less.These polar monomers only have low-pole, can be lower than about 30% and be preferably lower than about 20% or even lower content mix.
In certain embodiments, at least a derived from Isooctyl acrylate monomer, 2-EHA or n-butyl acrylate composition between the vinylformic acid and about 100% to about 96% between about 0 to about 6% of poly-(methyl) acrylic psa.A specific embodiment of the present invention is derived from the vinylformic acid between about 1% to about 2%, and at least a composition in the Isooctyl acrylate monomer between about 99% to about 98%, 2-EHA or the n-butyl acrylate.Specific embodiment derive about 1% to about 2% vinylformic acid, about 99% combination to about 98% n-butyl acrylate and methyl acrylate.
In other embodiments, poly-(methyl) acrylic psa derived from (methyl) acrylic acid hydroxy alkyl ester between about 0 to about 4%, and Isooctyl acrylate monomer, 2-EHA or n-butyl acrylate between about 100% to about 96% at least a composition.Specific embodiment is derived from (methyl) acrylic acid hydroxy alkyl ester between about 1% to about 2%, and at least a composition in the Isooctyl acrylate monomer between about 99% to about 98%, 2-EHA and the n-butyl acrylate.Specific embodiment derived from (methyl) acrylic acid hydroxy alkyl ester of about 1% to about 2%, with the composition of the combination of about 99% to about 98% n-butyl acrylate and methyl acrylate.
In certain embodiments, can be with the pressure sensitive adhesive component blend to form optically transparent mixture.In the polymeric constituent one or more can be crosslinked independently or crosslinked with general linking agent.This type of linking agent is included in the thermal cross-linking agent that is activated in the drying step process of the tackiness agent for preparing solvent coating.Such thermal cross-linking agent can comprise polyfunctional isocyanate, aziridine and epoxy compounds.In addition, UV-light or " UV " initiator can be used for crosslinked pressure sensitive adhesive.This type of UV initiator can comprise benzophenone and 4-acryloxy benzophenone.
Pressure sensitive adhesive can have viscosity inherently.If necessary, can in base material, add tackifier to form pressure sensitive adhesive.Available tackifier comprise (for example) rosin ester resin, aromatic hydrocarbon resin, aliphatic hydrocarbon resin and terpine resin.In general, preferably be selected from the light tackifier of hydrogenant rosin ester, terpenes or aromatic hydrocarbon resin.
Can add other material according to special requirement, comprise (for example) oil, softening agent, antioxidant, UV stabilizer, pigment, solidifying agent, polymeric additive, thickening material, dyestuff, chain-transfer agent and other additive, precondition is significantly not reduce the optical clarity of pressure sensitive adhesive.In certain embodiments, the softening agent of significant quantity is provided, be beneficial to dissociating and the required ionic movability of electrostatic dissipation characteristic of salt in the tackiness agent, for example can use amount greater than about 0.01 weight part (pbw), optional greater than the amount of about 0.10pbw and in certain embodiments greater than the amount (based on the acrylic adhesives meter of 100pbw) of about 1.0pbw.In addition, in certain embodiments, can provide the softening agent of significant quantity, for example less than the amount of about 20pbw and optional amount less than about 10pbw.In certain embodiments, softening agent can be beneficial to dissociating of salt in the tackiness agent and ionic movability.In certain embodiments, softening agent is selected from the solvable softening agent of vinylformic acid, comprises phosphoric acid ester, adipic acid ester, citrate, phthalic acid ester, the end capped low polyethylene oxide of phenyl ether.In general, preferably be non-hydrophilic plasticizer, for example do not contain those of oxirane repeating unit.Under high humidity and pyritous condition, non-hydrophilic plasticizer does not absorb measurable moisture content from atmosphere.For example, at room temperature non-hydrophilic plasticizer (for example in included example, using) show usually 0.01% or littler water in solubleness, more preferably 0.001% or littler.
Static inhibitor
Static inhibitor is by removing static charge or accumulating work by suppressing this electric charge.Can be used for static inhibitor of the present invention or organic solvable salt that dissociates comprises non-polymeric and polymer-type salt.Non-polymeric salt does not have repeating unit.In general, static inhibitor has constituted the anti-electrostatic pressure sensitive adhesive less than about 10% amount, optional anti-electrostatic PSA less than about 5% amount.In addition, static inhibitor has constituted the anti-electrostatic PSA greater than about 0.5% amount, optional anti-electrostatic PSA greater than about 1.0% amount.Even these materials are can not be in each system solvable also is organic soluble in selected system.In selected system, the salt that can dissociate is dissociated into charged ion.
Static inhibitor with dissociate strengthen the softening agent blending after, its usage quantity can be for 4% or still less, this significantly reduced the OCA cost and reduce static inhibitor and polaroid between the unfavorable interaction that may exist.In some preferred embodiments, anti-electrostatic salt is non-hydrophilic compounds.Non-wetting ability anti-electrostatic compound like this trends towards reducing the dependency of anti-electrostatic compounds property to humidity in improvement and pressure sensitive adhesive consistency.In certain embodiments, preferably negatively charged ion and positively charged ion all are organically, because the two all comprises carbon-containing group and nominal does not contain metal ion.In general, the amount of the static inhibitor that is added can not have a negative impact to the required optical clarity of anti-electrostatic pressure sensitive adhesive.In certain embodiments, mix the static inhibitor between about 0.05% to about 10% in the anti-electrostatic pressure sensitive adhesive, any number in this scope (for example 7%, 1.6% etc.) all can.
Choose the suitable static inhibitor that is used for given adhesive composition according to the positively charged ion and the anionic balance quality that constitute static inhibitor, to be implemented in the solubleness in the specific cure adhesive preparation.Thereby static inhibitor is organic soluble.
A kind of ion salt that compounds that is used to prepare the particular type of static inhibitor of the present invention for representing with general formula:
(R 1) t-vG +[(CH 2) qOR 2] vX -?????(I)
Each R wherein 1Comprise alkyl, alicyclic hydrocarbon, aryl, alkane alicyclic hydrocarbon, alkaryl, alicyclic alkyl, aralkyl, cyclophane alkyl and alicyclic ring aryl moiety, wherein this part can comprise one or more heteroatomss, for example nitrogen, oxygen or sulphur perhaps can comprise phosphorus or halogen (can be that fluoro is organic in essence therefore); Each R 2Comprise hydrogen or top at R 1Described part; G is nitrogen, sulphur or phosphorus; If G is a sulphur, then t is 3, if G is nitrogen or phosphorus then t is 4; If G is a sulphur, v is 1 to 3 integer, if perhaps G is nitrogen or phosphorus, then v is 1 to 4 integer; Q is 1 to 4 integer; And X is weak coordination organic anion, for example fluoro organic anion.R 1Alkyl preferably, R 2Preferred hydrogen, alkyl or acyl group (more preferably are hydrogen or acyl group; Most preferably be hydrogen).Detail is referring to U.S. Patent application 2003/0114560, and its content is incorporated this paper into way of reference.
The ion salt that is used to prepare the another kind of particular type of static inhibitor is represented with Formulae II:
(R 3) 4G’ +X -(II)
Each R wherein 3, independently, comprise alkyl, alicyclic hydrocarbon, aryl, alkaryl or aralkyl moiety, wherein G ' is N or P, wherein X -Be weak coordination organic anion.
The conjugate acid that suitable weak coordination organic anion has at least with the suitable acidity of hydrocarbyl sulfonic (for example has 1 hydrocarbyl sulfonic to about 20 carbon atoms; For example have 1 alkane, aryl or an alkarylsulphonic acid to about 8 carbon atoms; With in specific examples, be methane or tosic acid; Tosic acid most preferably).In general, conjugate acid is a strong acid.For example, the hammett acidity function H of anionic pure conjugate acid is less than about-7 (preferably less than about-10).
The example of suitable weakly coordinating anion comprises organic anion, as alkane, aryl and an alkarylsulphonic acid root; Alkane, aryl and alkaryl sulfate radical; Fluoridize and fluorizated four aromatic yl acid salts not; With fluorine-containing organic anion, for example fluoro aryl sulfonate radical, perfluoro alkyl sulfonic acid root, cyano group perfluor alkyl sulfonamide, two (cyano group) perfluor alkane alkylsulfonyl methide, two (perfluor alkane alkylsulfonyl) imines, cyano group-two-(perfluor alkane alkylsulfonyl) methide, two (perfluor alkane alkylsulfonyl) methide and three (perfluor alkane alkylsulfonyl) methide etc.
Remove the above those, the available positively charged ion also comprises (for example) alkali metal cation, as Li+, Na+ and K+.
The available ion salt can maybe can obtain from market by any existing method preparation.For example, can use the ion-exchange or the replacement(metathesis)reaction that are known in the art to prepare ion salt.More particularly, can be with relative acid blending in the aqueous solution of precursor salt and precursor metal salts or weakly coordinating anion.After the blending, required product precipitates or can preferably be extracted in the solvent.Product can be by filtering or separating by liquid phase/stratified liquid, can wash with water removing metal halide salt or hydrogen halide by product fully, and in a vacuum complete drying to remove whole volatile matter.Similarly replacement(metathesis)reaction can be carried out in organic solvent rather than water, and in this case, by-product salt preferably precipitates, and all products then are dissolved in the organic solvent (can use standard technique from wherein separated product) always.More detailed content is referring to U.S. Patent No. 6,372,829, and capable at the 8th hurdle 3-28 especially, it openly incorporates this paper into way of reference.An example of the commercially available salt of available is the 3M that derives from 3M company TMFluorad TMHQ-115, lithium (two) trifluoromethayl sulfonic acid imines.
The anti-electrostatic pressure sensitive adhesive
One embodiment of the present of invention are the acrylic pressure sensitive adhesive, it has and contains organic positively charged ion and (come from IVb family to VIIb family, preferably Vb family is to VIb family, Vb family most preferably) salt of the organic anion of son and strong Bu Langsi Taide acid (Bronsted acid), the wherein free point that disturbs adhesive power to the acrylic pressure-sensitive adhesive surface of this salt or its ion.One embodiment of the present of invention are acrylic PSA, and it has the salt of the organic anion that contains tetraalkylammonium cation and strong Bu Langsi Taide acid.Of the present invention is again acrylic PSA with embodiment, and it has the salt of the organic anion that contains inorganic cation and strong Bu Langsi Taide acid.
In certain embodiments, tackiness agent comprises and does not have surface-active positively charged ion and anionic salt, in this salt, through several hrs to several days or even longer time in, component can not be reduced to the viscosity of glass matrix below 50% of peak value levels of adhesion.In certain embodiments, tackiness agent can adhere to light polarizing film, and still can remove from glass surface after contacting at least about 7 days with the surface under 22 ℃ temperature and about 50% the relative humidity.These conditions can change independently, and for example, about 1 day to about 30 days, temperature was about 20 to about 30 ℃, and relative humidity is about 20% to about 90%.In certain embodiments, tackiness agent disclosed in this invention is an inert to light polarizing film basically, make it that enough initial viscosity and adhesive powers can be provided for the purpose that will reach, and still removable over time, and/or under the required exposure condition, do not make adhesive power be increased to unfavorable level.
In certain embodiments, by form PSA and with its with the static inhibitor blend forming the anti-electrostatic blend, thereby prepare the anti-electrostatic pressure sensitive adhesive.Before or after polyreaction, form pressure sensitive adhesive by the blend pressure sensitive adhesive component.In certain embodiments, with pressure sensitive adhesive component further with the light trigger blend.Suitable light trigger comprises: for example from the Irgacure651 of the Ciba Specialty Chemicals of New York Tarrytown.The processing that at first outgases in nitrogen of pressure sensitive adhesive monomer uses suitable source of radiation (for example ultra-violet lamp) irradiation for some time to form slurry then.Slurry has the viscosity of about 200 centipoises (0.2Pa-s) to about 3000 centipoises (3Pa-s) usually.Then slurry is mixed with anti-electrostatic reagent, linking agent (polyfunctional acrylic ester of crosslinked slurry) and optional softening agent.The binder composition of gained is coated on the antiseized liner, and further uses UV-irradiation, produce the optically transparent tackiness agent of complete polymeric.
With static inhibitor with less than about 10%, optional less than about 5% or even lower weight % be incorporated in the slurry.In addition, with static inhibitor with greater than about 0.5%, and optional greater than about 1.0% or even bigger weight % be incorporated in the slurry.Can use any currently known methods, for example shake, stir or mix, with static inhibitor and slurry blend.The combination of this slurry and static inhibitor makes the anti-electrostatic pressure sensitive adhesive of gained have required optical property after suitably solidifying.
In the solvent-borne type pressure sensitive adhesive, the solution from organic solvent applies PSA drying then.Solvent-borne type PSA is crosslinked in the drying treatment process, perhaps in some cases can be crosslinked behind drying step.This type of linking agent is included in activatory thermal cross-linking agent in the drying step of tackiness agent of preparation solvent coating.Such thermal cross-linking agent can comprise polyfunctional isocyanate, aziridine and epoxy compounds.In addition, can use the light-triggered linking agent of ultraviolet.The light-triggered linking agent of this type of ultraviolet can comprise benzophenone and 4-acryloxy benzophenone.
For further optimizing the bond properties of optically transparent tackiness agent, can in optically transparent tackiness agent of the present invention, mix short adhesive additive, for example silane and titanate.Examples of such additives can by with substrate in silanol, hydroxyl or other reactive group between combine the adhesive power that promotes between tackiness agent and the substrate (being similar to glass and the cellulose triacetate of LCD).But silane can only have alkoxy substituent with titanate on Si that is connected tackiness agent copolymerization or interaction group or Ti atom.Alternatively, but silane and titanate can have alkane and alkoxy substituted simultaneously on Si that is connected to tackiness agent copolymerization group or interaction group or Ti atom.But tackiness agent copolymerization group is generally acrylate group or methacrylate based group, but also can use vinyl and allyl group.Alternatively, silane or titanate also can react to each other with the functional group in the tackiness agent, for example (methyl) acrylic acid hydroxy alkyl ester.In addition, silane or titanate also can have provides the one or more groups that carry out strong interaction with binder matrix.The example of this strong interaction comprises that hydrogen bond, ionic interaction and acidic group interact.
In certain embodiments, preferably one or more in softening agent, sequestrant and the polyvalent metal ion are minimized even eliminate.In certain embodiments, inorganic/organic salt combination (for example above-described HQ-115) can be used and the optional sequestrant that do not contain with PSA as herein described and optional non-hydrophilic plasticizer.In certain embodiments, when using alkali metal cation in the salt, also use non-hydrophilic plasticizer.
In certain embodiments, select sequestrant, for example, in appropriate organic solvent (as ethyl acetate, toluene, methyl ethyl ketone, acetone or alcohols), have acceptable solubleness and have and those of the acceptable consistency of PSA.Suitable sequestrant example comprise have the oxalate group, those compounds of diamine groups, poly-carboxyl or β ketone groups, these compounds can use separately or use with the form of mixture.More particularly, example comprises oxalic acid diethyl ester, dimethyl oxalate, dibutyl oxalate, oxalic acid di tert butyl carbonate or two (4-methyl-benzyl-1) barkite; Quadrol, 1, diaminobutane, quadrol-N, N, N ', N ' tetraacethyl (EDTA), N, N, N ', N "; N "-diethylene triaminepentaacetic acid(DTPA) (DTPA), 1,4,7,10-tetraazacyclododecanand-N, N ', N ", N " ' tetraacethyl (DOTA), 1,4,7,10-tetraazacyclododecanand-N, N ', N " nitrilotriacetic (DO3A), trans (1,2)-hexalin diethylene triaminepentaacetic acid(DTPA) and N, N-dicarboxyl methylglycine.Those skilled in the art should be understood that this type of sequestrant can use the level of mixing PSA with increase salt with metal-salt, yet this combination has changed the fundamental characteristics of PSA, thereby it is not suitable for all application.This section will be discussed.
In certain embodiments, can use one or more ester plasticizers, for example Diethylene Glycol two-2-ethylhexanoate, TEG two-2-ethylhexanoate, polyoxyethylene glycol two-2-ethylhexanoate, triethylene glycol diethyl capronate, polyoxyethylene glycol diethyl butyric ester, polypropylene glycol diethyl capronate, triethylene glycol dibenzoate, polyethylene glycol dibenzoate, polypropylene glycol dibenzoate and polyoxyethylene glycol-2-ethylhexyl benzoic ether with one or more ehter bonds.In other embodiments, do not use such softening agent.This section will be discussed.
In certain embodiments, PSA does not contain one or more in sequestrant, non-hydrophilic plasticizer and the quaternary ammonium salt, has reported that before this these materials can be used as PSA.
Can binder composition be coated on the suitable flexible back lining materials easily to produce the flaky material that tackiness agent applies by any known paint-on technique.Flexible back lining materials can be any material that is conventionally used as band backing, blooming, antiseized liner or any other flexible materials.The representative instance that is used as the flexible back lining materials band backing, that be applicable to binder composition comprises those that made by paper, plastic film (for example polypropylene, polyethylene, urethane, polyvinyl chloride, polyester (for example polyethylene terephthalate), cellulose acetate and ethyl cellulose).Some flexible backings can have coating, for example can apply antiseized liner with low adhesive power component (for example siloxanes).In certain embodiments, the second release liner sheet can be laminated to the exposed face of antistatic adhesive agent, this antistatic adhesive agent has been coated on the first antiseized liner.The first antiseized liner or the second antiseized liner or the two can show electrostatically dissipative to a certain degree.
Pressure sensitive adhesive of the present invention can directly be coated on the one or both sides of optical element (for example polaroid).Polaroid can comprise other layer, for example anti-photosphere, protective layer, reflecting layer, phase delay layer, wide-angle layer of compensation and the brightness enhancing layer of dazzling.In certain embodiments, pressure sensitive adhesive of the present invention can be coated on the one or both sides of liquid crystal cell.It can also be used for polaroid-bindnig to liquid crystal cell.
Pressure sensitive adhesive of the present invention can apply with multiple known paint-on technique (for example roller coat, spraying, blade coating, mould coating etc.).
The pressure sensitive adhesive of gained has required antistatic performance.In general, surface resistivity is less than 1 * 10 13Ohm-sq.In certain embodiments, surface resistivity is less than 1 * 10 11Ohm-sq.In addition, under low humidity condition and super-humid conditions, PSA has antistatic performance, and does not cause the decline of any rotten or antistatic performance of tackiness agent self.
The volume specific resistance of tackiness agent disclosed in this invention or resistance are usually less than about 1 * 10 11Ω-cm passes that its thickness (also being called " z-direction ") measures.
The volume specific resistance of tackiness agent disclosed in this invention or resistance are usually less than about 1 * 10 11Ω-cm measures on its plane.As used herein, the tackiness agent plane is the x-y direction, or perpendicular to the direction of adhesive thickness.In certain embodiments, at the resistance (Ω) of z-and/or x-y direction much smaller than 1 * 10 11Ω-cm.
The moisture that absorbs in the pressure sensitive adhesive may cause producing bubble in tackiness agent, changes its antistatic performance or produces mist degree.Organic soluble salt especially is the organic soluble salt of non-wetting ability, absorbs less moisture, thereby can keep stable in multiple environment.Similarly, non-hydrophilic plasticizer absorbs few moisture or does not absorb moisture, and the tackiness agent of optically transparent and ambient stable is provided.The twice of (20 ℃ time 50% humidity) surface resistivity when usually preferably, the surface resistivity during low humidity (23 ℃ time 23% humidity) does not exceed high humidity.
In addition, organic antistatic agents (as mentioned above) is available and is stable in anti-electrostatic PSA of the present invention.Under certain conditions, inorganic and metallic cation salt can be tending towards precipitation and realize being separated with pressure sensitive adhesive matrix.Under low humidity or do not exist under the condition of solubilising component especially truely, for example comprise the polyethylene oxide of softening agent and metal ion-chelant softening agent or additive.Given this reason, usually preferred organic cation and negatively charged ion.
Anti-electrostatic pressure sensitive adhesive of the present invention shows required optical property, and tackiness agent for example disclosed in this invention has higher transmittance and lower mist degree than the substrate of choosing.Therefore, PSA goods of the present invention have and essentially identical transmittance of independent backing and mist degree.In other embodiments, anti-electrostatic PSA has the opaqueness lower than substrate, for example less than 1%; In a particular embodiment, less than 0.6%.In multi-layer product, common every layer all can be reduced transmittance.
In the time of in adding multilayered structure to, anti-electrostatic pressure sensitive adhesive of the present invention can further not reduce optical property usually.For example, have greater than 88% transmittance and less than the thick polyethylene terephthalate sheet of 25 μ m of 5% mist degree after PSA of the present invention is placed on the backing of this polyethylene terephthalate, still have greater than 88% transmittance with less than 5% mist degree.In such embodiments, tackiness agent will have greater than 88% the transmittance of (for example 89% or higher).In certain embodiments, mist degree is less than 4%; And in certain embodiments, mist degree is less than 2%.The opaqueness of the anti-electrostatic pressure sensitive adhesive of some embodiment is usually less than 1%, more preferably is lower than about 0.6%.Can use microslide to measure these optical signatures: elder generation is laminating adhesive not, then laminating adhesive on slide glass, relatively twice result.
In general, if LCD does not have to damage and do not retain a large amount of adhesive residue on LCD substantially when removing tackiness agent, then be coated to pressure sensitive adhesive on the LCD and can regard as and can reprocess.Can reprocess pressure sensitive adhesive show usually have at least about 2, at least about 3 or even at least about 5 from 180 ° of peel adhesion peeling off on glass (unit is N/dm, and all is to place after 1 minute under the room temperature).The slip resistance of the anti-electrostatic pressure sensitive adhesive of gained is at least 1000 minutes.Can reprocess pressure sensitive adhesive shows to have and is not higher than about 75,65,50,40,30 or even lower from 180 ° of peel adhesion peeling off on glass (unit is N/dm, and all be 65 ℃ place after 1 hour down).
It should be noted that poly-(oxirane) softening agent is possess hydrophilic property inherently, therefore, the OCA that comprises poly-(oxirane) demonstrates low weather resistance to moisture-sensitive and in high temperature and high humidity environment.Therefore, the tackiness agent that comprises this type of material is not applicable to that very LCD uses.
Because anti-electrostatic OCA of the present invention can directly contact with polaroid; so; must not have such component in the tackiness agent: with other any layer unfavorable interaction that is enough to cause degraded of tri acetyl cellulose (TAC) skin or polaroid, this degraded can weaken the polaroid performance undesirably.In addition, the iodine in tackiness agent of the present invention and the polaroid do not interact or not the polarisation-affecting sheet orientation and cause the bleaching of polaroid.
The present invention can be used for the anti-electrostatic pressure sensitive adhesive applications, for example is used for the LCD assembly.
Further specify target of the present invention and advantage below in conjunction with example, and the certain material of being quoted in these examples and consumption and other condition and details should not be construed as and limit the present invention undeservedly.
Example
Do not indicate in addition if having, material derives from chemical supply corporation, for example the Aldrich of Milwaukee, the state of Wisconsin (aldrich) company.
Material
Figure G2008800119066D00171
The preparation [(C of nine fluorine butane sulfonic acid TBuAs 4 H 9 ) 4 N + ] [(C 4 F 9 SO 3 - )]
By U.S. Patent No. 6,372, the capable described general procedure of the 8th hurdle 3-28 among the 829B1 is by tetrabutylammonium chloride and nine fluorine butane potassium sulfonates (FR2225, the 3M company of Minnesota State St.Paul) prepared in reaction, nine fluorine butane sulfonic acid TBuAs.
Dodecyl methyl is two-two (fluoroform sulphonyl) the imido systems of (2-hydroxyethyl) ammonium Be equipped with.[C 12 H 25 N + (CH 3 )(CH 2 CH 2 OH) 2 ][ - N(SO 2 CF 3 ) 2 ]
Dodecyl methyl is two-and two (fluoroform sulphonyl) imide preparation methods are as follows for (2-hydroxyethyl) ammonium: 75%ETHOQUAD C/12 (323.5g/ mole) the solid aqueous solution that under agitation adds 55.0g (0.127 mole) among the 36.38g in 70ml water (0.127 mole) HQ-115.Room temperature (25 ℃) is after following 2 hours, with 70ml dichloromethane extraction reactant.With 40ml water flushing dichloromethane layer, concentrate 3 hours at 60-120 ℃ with vacuum ejector then, produce the light brown of 70.54g (94.3%), transparent sticky product.
Two (fluoroform sulphonyl) the imido preparations of three-(normal-butyl) ammonium methyls. [(C 4 H 9 ) 3 (CH 3 )N + ][ - N(SO 2 CF 3 ) 2 ]
By U.S. Patent No. 6,372, the capable described general procedure of the 8th hurdle 3-28 among the 829B1 is by tributyl-methyl phosphonium ammonium chloride and two (fluoroform sulphonyl) imides of two (fluoroform sulphonyl) imide li (3M HQ115) preparation three-(normal-butyl) ammonium methyls.
Synthesizing of representative PSA solution
In 1 liter bottle, inject VAZO67 (0.2g), n-butyl acrylate (BA) (98g), 4-hydroxyl acrylic butyl ester (4HBA) (2g) and ethyl acetate (150g).Nitrogen was fed in the solution 10 minutes.Bottle seals in nitrogen atmosphere and was placed on then in the water-bath that is heated to 58 ℃ 24 hours, and bottle during this period rolls in water-bath.At last, in bottle, add ethyl acetate (210g) and toluene (40g) to produce 20% solid solution.
Testing method
Peel off the bonding strength test
Bonding strength is peeled off in following test: (thickness=2.54cm) be laminated on the preprepared polyester film (38 μ m) removes initial antiseized liner from tackiness agent, then binder layer is incorporated on the LCD sheet glass with adhesive sample.Contact after 1 minute, have the adhesive sample of polyester backing, peel off with angle 30cm/ minute speed of 180 degree.Be labeled as in the table as a result in the hurdle of initial glass bounding force and shown the required power of adhesive sample that removes.Except as otherwise noted, otherwise sample does not stay any resistates on glass when LCD glass removes.Some adhesive samples that are laminated to LCD polyester backing on glass were placed in the baking oven under 65 ℃ 1 hour.Make sample be cooled to room temperature, and repeat the aforesaid bonding strength test of peeling off.Show that from the peeling force variation of initially adhering to time value and 1 hour high temperature exposure value the adhesive power of band increases and the removable time limit is longer.Except as otherwise noted, tackiness agent totally removes from the LCD sheet glass otherwise after described high temperature exposure.
Durability test
Adhesive sample is laminated to " polaroid " film, initial antiseized liner is removed and binder layer is bonded to LCD glass.Laminated sample is placed in the baking oven that remains under 65 ℃ and 90% relative humidity week ages at most.Once in a while sample is removed the visual inspection defective from baking oven.If the defective of not observing, the sample deciding grade and level is sent it back to baking oven then immediately for " qualified ".If any sample is presented at the adhesive interface of tackiness agent or inner indenture, the visible bubble of forming of tackiness agent, or shows that polaroid is peeled off from LCD glass and cause edge perk or polaroid/tackiness agent/LCD glass assembly to separate fully, all it is indicated.Indenture and air bubble problem can be improved by meticulous adjustment adhesive formula, and delamination then is unacceptable failure mode.Also to observe the transmission of visible light of OCA, not be " transparent ", if tackiness agent is than initial appearance degradation or muddiness then define the level and be " bluring " if observe variation then define the level.
Surface resistivity
Measure the surface resistivity of adhesive sample according to ASTM D257.Sample is adjusted 24 hours under 23 ℃ and 23% relative humidity condition after, the tackiness agent sample is placed between two electrodes of Keithly 8009 testing apparatuss (the Keithley Instruments Inc. of Ohio Cleveland), makes it be exposed to 60 seconds under the 500v electromotive force.Be exposed to immediate record surface resistivity in back under the 500v electromotive force.
The test of DV volume resistance
The thick adhesive sample of 25 μ m is coated on the aluminium base of the about 50mm of diameter.Then, two diameters parallel, concentric aluminium electrode of being 9.41mm is placed on respectively on the apparent surface of tackiness agent/aluminium sample.Use the DC resistance of DC Keithly 6515A electrometer (the Keithley Instruments of Ohio Cleveland) three samples of independent measurement.Use the volume specific resistance under the measuring resistance calculating 100vDC between electrode diameter, adhesive thickness and two electrodes.
Mist degree and transmittance
The adhesive sample that 25 Xie are thick is laminated to the thick Melinex of 25 μ m TM454 polyester films (E.I.Du Pont Company of Delaware State Wilmington), laminated mode must guarantee not produce air bubble between film and binder layer.With the Plain Micro slide glass (the Dow Corning of state of Michigan Midland) of 75mm * 50mm with isopropyl alcohol three times after, use the hand roller that it is laminated to adhesive sample, to guarantee not produce air bubble between tackiness agent and the glass slide.(Columbia MD) measures transmission percentage ratio (%) and mist degree to use Model 8870BYK Gardner TCS PLUS spectrophotometer.Use Melinex 454 and microslide interlayer to measure background.Then, can in spectrophotometer, on the laminated thing of film/adhesive/glass, directly obtain the % transmittance and the mist degree of adhesive sample.
Polaroid bleaching test
Adhesive sample is laminated on two light polarizing film.Laminated sample is placed on a week in the baking oven that remains under 65 ℃ and 90% relative humidity.One in these samples are placed on another, and its polarization axle is 90 degree.Have light to leak if observe through two samples, then this tackiness agent/polaroid combination is judged to be unsettled.Stable tackiness agent/polaroid combination does not allow two samples of light transmission to leak.
Table 1: pressure sensitive adhesive (mol ratio)
??IOA ??AA ??BA ??AcM ??4HBA ??EA ??MA ??HEA
??PSA?1 ??98 ??2 ??--- ??--- ??--- ??--- ??--- ??---
??PSA?2 ??--- ??2 ??98 ??--- ??--- ??--- ??--- ??---
??PSA?3 ??96 ??--- ??--- ??4 ??--- ??--- ??--- ??---
??PSA?4 ??--- ??--- ??96 ??--- ??4 ??--- ??--- ??---
??PSA?5 ??--- ??--- ??88 ??--- ??--- ??10 ??--- ??2
??PSA?6 ??--- ??--- ??98 ??--- ??--- ??--- ??--- ??2
??PSA?7 ??--- ??--- ??58 ??--- ??--- ??--- ??40 ??2
??PSA?8 ??--- ??--- ??88 ??--- ??--- ??--- ??10 ??2
The IOA=Isooctyl acrylate monomer, AA=vinylformic acid, the BA=butyl acrylate, the AcM=acrylamide, 4HBA=4-hydroxyl acrylic butyl ester, the EA=ethyl propenoate, the MA=methyl acrylate, HEA=2-hydroxyl acrylic ethyl ester, "---" use of expression.
The preparation of anti-electrostatic OCA sample
By being put into wide-necked bottle, linking agent, static inhibitor and the optional softening agent of PSA solution, aequum prepare coating solution.Wide-necked bottle is placed on mechanical roller last 30 minute.Solution is coated on the antiseized liner of silication polyester, and in being set at 70 ℃ forced ventilation baking oven heating coated sample 30 minutes.About 25 μ m are thick for final adhesive sample.
Table 2: tackiness agent
Figure G2008800119066D00211
Umber among the per 100 parts of solid PSA of PPH=
* example 9 comprises 3-(glycidoxypropyl)-Trimethoxy silane of 0.05PPH
Table as a result
Example Initial glass adhesive power (N/dm) 65 ℃ of adhesive powers (N/dm) after following 1 hour Surface resistivity (ohm-sq) The DC volume specific resistance (Ω-cm) The polaroid durability test
??1 ??13.8 ??15.0 ??3.6E+09 ??---- Transparent
??2 ??18.9 ??19.0 ??2.7E+09 ??---- Transparent
??3 ??11.5 ??12.8 ??9.2E+09 ??---- Can
??4 ??8.6 ??9.1 ??7.8E+09 ??---- Indenture
??5 ??7.4 ??8.0 ??6.3E+09 ??---- Bubble
??6 ??23.4 ??28.2 ??6.0E+10 ??---- Can
??7 ??14.0 ??20.7 ??4.6E+10 ??---- Can
??8 ??22.8 ??25.9 ??1.3E+10 ??1.64E+09 Can
??9 ??18.5 ??22.7 ??7.2E+10 ??5.56E+09 Can
??10 ??33.4 ??49.7 ??4.3E+09 ??---- Bubble
??11 ??25.2 ??50.8 ??6.0E+08 ??---- Bubble
??12 ??31.3 ??43.6 ??2.8E+09 ??---- Can
??13 ??22.1 ??48.5 ??2.2E+09 ??---- Transparent
??14 ??23.1 ??35.9 ??9.8E+09 ??---- Can
??15 ??13.8 ??25.0 ??5.6E+09 ??---- Can
??16 ??11.7 ??33.6 ??4.8E+09 ??---- Indenture
??17 ??10.1 ??18.9 ??4.1E+09 ??---- Bubble
??18 ??18.8 ??23.3 ??3.24E+11 ??4.48E+09 Fuzzy
Comparative example 1 No adhesive power No adhesive power ??7.8E+11 ??---- Fuzzy
Comparative example 2 ??45.6 ??72.9 ??1.8E+10 ??---- Bubble
Comparative example 3 ??24.3 ??62.3 ??9.4E+11 ??---- Transparent
Comparative example 4 ??15.1 ??19.5 ??5.0E+13 ??---- Can
Comparative example 5 ??17.5 ??47.5 ??1.09E+10 ??2.27E+09 Peel off
Comparative example 6 ??--- ??--- ??9.9E+10 ??---- Fuzzy
Comparative example 1 shows as no adhesive power, but can be by reducing salts contg and/or adding softening agent and improved, shown in above-mentioned example.
Under the prerequisite that does not deviate from scope of the present invention and principle, various modifications of the present invention and change will be conspicuous concerning those skilled in the art, and should be appreciated that the present invention should not be limited to exemplary embodiment mentioned above undeservedly.

Claims (29)

1. optically transparent indicating meter level tackiness agent, it comprises:
Crosslinked acrylic psa;
Organic soluble and can dissociated salt; And
Non-hydrophilic plasticizer,
Wherein said tackiness agent is an electrostatically dissipative, and transmission of visible light be at least about 80% and mist degree be lower than about 10%.
2. tackiness agent according to claim 1, it also comprises short adhesive additive.
3. tackiness agent according to claim 2, wherein said short adhesive additive is selected from silane and titanic acid ester.
4. tackiness agent according to claim 1, wherein said acrylic psa comprises the reaction product of following material, and described material is one or more vinylformic acid or (methyl) acrylate monomer and optional comonomers.
5. tackiness agent according to claim 1, wherein said acrylic psa comprises one or more following monomeric reaction product, and described monomer is selected from (methyl) butyl acrylate, (methyl) 2-EHA, (methyl) ethyl propenoate, (methyl) methyl acrylate, (methyl) vinylformic acid n-propyl, (methyl) isopropyl acrylate, (methyl) tert-butyl acrylate, (methyl) vinylformic acid pentyl ester, (methyl) vinylformic acid n-octyl, (methyl) Isooctyl acrylate monomer, (methyl) vinylformic acid ester in the different ninth of the ten Heavenly Stems and (methyl) vinylformic acid 2-ethyl butyl ester.
6. tackiness agent according to claim 1, wherein said salt comprises alkali metal cation and organic anion.
7. tackiness agent according to claim 1, wherein said salt comprises organic cation and organic anion.
8. tackiness agent according to claim 1, described in salt be lower than about 10 effectively providing 11The amount of the adhesive surface resistivity level that Ω is every square provides; And/or be lower than about 10 can effectively providing 11The amount of the tackiness agent volume specific resistance level of Ω-cm provides.
9. tackiness agent according to claim 1, wherein said salt is to provide based on the weight of described acrylic psa about 0.5 amount to about 5 weight %.
10. tackiness agent according to claim 1, wherein said salt and softening agent are lower than 10 effectively providing to be respectively 11The every sum of squares 10 of Ω 11The adhesive surface resistivity level of-cm and the amount of volume specific resistance level provide.
11. tackiness agent according to claim 1, wherein said salt comprises the negatively charged ion of strong Bu Langsi Taide acid, or is selected from the negatively charged ion of sulfonate radical, sulphonamide, sulfimide.
12. tackiness agent according to claim 1, wherein said salt comprises the anionic group that is selected from methide and borate.
Be selected from cationic positively charged ion 13. tackiness agent according to claim 1, wherein said salt comprise, described positively charged ion is from IVb to VIIb family, Vb to VIb family, An, Phosphonium, sulfonium, lithium, sodium and potassium in the periodictable.
14. tackiness agent according to claim 1, wherein said salt comprises non-hydrophilic compounds.
15. comprising, tackiness agent according to claim 1, wherein said salt do not have surface-active negatively charged ion and positively charged ion.
16. tackiness agent according to claim 1, the described tackiness agent that wherein adheres to polarizing coating still can remove from described surface after contacting at least about 7 days with glass surface under 22 ℃ temperature and about 50% the relative humidity.
17. tackiness agent according to claim 1, wherein said salt comprises mineral ion, and described softening agent is made up of one or more non-hydrophilic plasticizer substantially.
18. tackiness agent according to claim 1, wherein said softening agent provides with significant quantity, randomly is the softening agent based on the acrylic adhesives meter 0.01 to about 10pbw of 100 weight parts (pbw).
19. tackiness agent according to claim 1, wherein said softening agent are selected from the soluble softening agent of vinylformic acid, comprise phosphoric acid ester, adipic acid ester, citrate, phthalic acid ester and their combination.
20. tackiness agent according to claim 1, wherein said salt are selected from two (perfluor alkane alkylsulfonyl) imines and the perfluoro alkyl sulfonic acid tetra-allkylammoniums of tetra-allkylammonium.
21. it is inert that tackiness agent according to claim 1, wherein said tackiness agent are gone up polarizing coating substantially.
22. an optically transparent indicating meter level tackiness agent, it is composed of the following components basically:
Crosslinked acrylic psa; And
It is organic soluble and can dissociated salt,
Wherein said salt comprises alkali metal cation and organic anion.
23. an optically transparent indicating meter level tackiness agent, it is composed of the following components basically:
Crosslinked acrylic psa;
Organic soluble and can dissociated salt; And
Short adhesive additive,
Wherein said salt comprises alkali metal cation and organic anion.
24. a multilayer polaroid, it comprises according to claim 1,22 or 23 described tackiness agents, chooses wantonly and wherein all provides described tackiness agent in the polarizing coating both sides.
25. multilayer polaroid; it comprises according to claim 1,22 or 23 described tackiness agents, and wherein said polaroid also comprises and is selected from anti-one or more layers of dazzling in photosphere, protective layer, reflecting layer, phase delay layer, wide-angle layer of compensation and the brightness enhancing layer.
26. a liquid-crystal display, it comprises according to claim 1,22 or 23 described tackiness agents; Polaroid; And liquid crystal cell, choose wantonly and wherein all provide described tackiness agent in described liquid crystal cell both sides.
27. a method for preparing optically transparent indicating meter level tackiness agent, this method comprises:
At least a acrylic monomer and optional at least a comonomer and optional light trigger are provided;
With described monomer and organic soluble dissociate salt and linking agent blend, to form the adhesive precursor composition;
Described adhesive precursor composition is provided on the first antiseized liner; And
Activate described linking agent forming crosslinked acrylic psa,
Wherein said tackiness agent is an electrostatically dissipative, and the transmission of visible light of optional wherein said tackiness agent be at least about 80% and mist degree be lower than about 10%.
28. also comprising, method according to claim 27, this method provide non-hydrophilic plasticizer and with described softening agent and described monomer, salt and/or the blend of adhesive precursor composition.
29. method according to claim 27, this method also comprise the second release liner sheet is laminated to described tackiness agent with the described first antiseized liner facing surfaces on, the optional wherein said first and/or second antiseized liner is an electrostatically dissipative.
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